Research On Synthesis Of Ethyl Acetate Through Reactive Distillation Process Intensified By Microwave Irradiation

Given the limitations of reactive distillation process, such as slow esterificationreaction rate and low thermal efficiency, a new process coupling intensificationtechnology-microwave reactive distillation technology was developed by usingadvantages of microwave to accelerate the chemical reaction rate and high efficiencyand energy saving in microwave dielectric heating. So the conventional reactivedistillation process could be intensified through microwave. The synthesis of ethylacetate reaction system was selected as research object, and the process intensified bymicrowave irradiation of reactive distillation esterification and its related contentswere studied systematically.In order to quickly, accurately and conveniently determine the composition of theresearch components, for instance water, ethanol, acetic acid and ethyl acetate. A gaschromatography quantitative analysis method combined with the piecewise fittingwas established in this paper. And it effectively overcame the inaccurate of areanormalization method and the incovenient of titration. So the relative standarddeviation of four components in mass fraction is0.08%~0.35%. This provides areliable analysis for the next study of reaction kinetics and reactive distillationexperiment.To reveal the microwave radiation effect on reaction kinetics, a set of microwavereaction apparatus was designed. And the microwave power, catalyst dosage andreaction temperature was investigated. Based on that, the NKC-9and Amberlyst15were selected as catalyst to comparative research the heterogeneous esterificationreaction kinetics in catalytic synthesis of ethyl acetate under microwave andconventional heating. The experimental results show that under microwave heating,the reaction rate is enhanced and the reaction kenetics has been changed, whichindicates the existence of microwave non-thermal effect. This provides basal reactionkinetics data for the following reactive distillation experiment and simulation.The microwave and conventional batch reactive distillation was comparativestudyed to explore the process intensified by microwave radiation. And themicrowave power, operating reflux ratio and acetic acid feed flow rate wereinvestigated. The results show that under microwave radiation, the ethyl acetate purityand ethanol conversion are respectively increased by6.88%and5.71%comparision with conventional heating. The experimental process was simulated and simulationresults accord with the experiment well by using Aspen Batch DistillationThe compared research on microwave and conventional continuous reactivedistillation esterification were performed. And the microwave power, heating jacketpower, reflux ratio and total feed flow rate were investigated. The thermal efficiencyunder microwave and conventional were made a comparison. The results show thatunder microwave radiation, the ethyl acetate purity increases from81.15%to83.52%and the average increase ratio is1.48%comparision with conventional condition. Themaximum improvement ratio of thermal efficiency under microwave is23.99%comparision with conventional experiment. At last, experimental process ofcontinuous reactive distillation was simulated and simulation was consistent with theresults by using Aspen Plus non-equilibrium stage model.